Water → HCID 13577659、化合物

HRID 1589210ノート

反応式

HRID 1589210 の反応式
[NH2:1][C:2]1[C:7]([C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][C:18](OCC)=[O:19].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:1][C:2]1[C:7]([CH:8]([OH:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][CH2:18][OH:19]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 13577656HCID 13577656、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 13577659HCID 13577659、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 15.85 g (0.05 mole) of 2-amino-3-benzoyl-5-chlorobenzeneacetic acid, ethyl ester dissolved in 100 ml of dry tetrahydrofuran was added dropwise to a suspension of 4.0 g (0.105 mole) of lithium aluminum hydride in 50 ml of dry tetrahydrofuran. Gentle reflux was maintained during the addition. Reflux was continued for 2 hours after completion of the addition. The mixture was cooled and carefully treated with 4 ml of water, 4 ml of 15% sodium hydroxide and 12 ml of water. The resulting mixture was filtered, the filtrate stripped and the resulting residue recrystallized from toluene. The titled compound, 10.5 g (70%) having a m.p. of 130°-132° C. was obtained.

後処理

  1. temperatureGentle reflux
  2. temperaturewas maintained during the addition
  3. temperatureReflux
  4. additionafter completion of the addition
  5. temperatureThe mixture was cooled
  6. filtrationThe resulting mixture was filtered
  7. customthe resulting residue recrystallized from toluene
  8. customwas obtained

出典と根拠

ORDレコード
ord-407d037d476946e0858e390a2667ff4e
出典データセット
uspto-grants-1986_02
特許番号
US04568695

反応ノート

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